Acetic Acid → 3-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

HRID 1983453ノート

反応式

HRID 1983453 の反応式
[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=C(C#N)[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2.[C:21]([OH:24])(=[O:23])[CH3:22].O.S(=O)(=O)(O)O>C(OCC)(=O)C>[S:1]1[C:5]([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=[C:22]([C:21]([OH:24])=[O:23])[CH:13]=3)[NH:8][N:7]=2)=[CH:4][C:3]2[CH:17]=[CH:18][CH:19]=[CH:20][C:2]1=2

参加物

6

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 1118Sulfuric AcidHCID 222607323-Benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile

生成物 1

HCID 222606653-Benzo[b]thiophen-2-yl-1H-5-indazolecarboxylic Acid

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
110 °C

実験手順

To 288 mg of 3-benzo[b]thiophen-2-yl-1H-5-indazolecarbonitrile were added 3 ml of glacial acetic acid, 1 ml of water and 0.8 ml of concentrated sulfuric acid, and the mixture was stirred at 110° C. for 4 hours. After standing to cool, the mixture was added with 120 ml of ethyl acetate, sequentially washed with water and brine, dried over anhydrous magnesium sulfate. After filtering the organic layer through a silica gel pat, the solvent was evaporated, to give 307 mg of the title compound as ocher yellow crystals.

後処理

  1. temperatureto cool
  2. washsequentially washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationAfter filtering the organic layer through a silica gel pat
  5. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-1423addcda24429d8681f272736c380b
出典データセット
uspto-grants-2009_06
特許番号
US07541376B2

反応ノート

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